CN101082611B - light-catalyzed reaction concentrating thermal decomposition suction automatic sampling instrument - Google Patents
light-catalyzed reaction concentrating thermal decomposition suction automatic sampling instrument Download PDFInfo
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- CN101082611B CN101082611B CN2007100290593A CN200710029059A CN101082611B CN 101082611 B CN101082611 B CN 101082611B CN 2007100290593 A CN2007100290593 A CN 2007100290593A CN 200710029059 A CN200710029059 A CN 200710029059A CN 101082611 B CN101082611 B CN 101082611B
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Abstract
The invention discloses an automatic sampling element of optical catalyzing reaction-condensing heat desorption, which comprises the following parts: optical catalyst reacting device, condensing heat desorbing sampling device and control board, wherein the optical catalyzing reacting device is composed of optical source, calandria A, heat electric couple A, optical catalyst coating, optical catalyzing reacting pipe, electromagnetic valve I, electromagnetic valve II, electromagnetic vale II, electromagnetic vale IV, gas inlet pipe, gas carrying pipe A, blow-down pipe A and sampling pipe; the condensing heat desorbing sampling device contains heat desorbing cavity, calandria B, heat electric couple B, condensing pipe, mobile insulating sleeve, electromagnetic valve V, electromagnetic valve VI, sampling needle, gas carrying pipe B and blow-down pipe B; the control board is composed of CPU microprocessor unit, electromagnetic valve driving circuit, AC driving mode A-C, temperature signal A-to-D switching circuit and RS232 serial communication circuit to connect electrically. The invention integrates reacting, sampling, sample condensing, desorbing and sampling technique through automatic technique, which controls the reacting parameter to do on-line reaction and detection automatically.
Description
(1) technical field
The present invention relates to a kind of light-catalyzed reaction-concentrated thermal desorption automatic sampling instrument that online detection photocatalysis to degrade organic matter changes that is applied to, relate to light-catalyzed reaction, concentrate thermal desorption technology and automatic control technology.
(2) background technology
At present, the photocatalysis to degrade organic matter technology comes into one's own on environmental protection, chemical field day by day.Measure the performance of catalysis material degradation of organic substances, normally adopt special purpose reactor to carry out light-catalyzed reaction, gather reacted gaseous sample then and detect by gas chromatography or spectrographic technique.Because organic variation is micro-in the light-catalyzed reaction process, and this method reaction is to separate with detecting, so the test result reappearance is relatively poor, complex operation can not carry out online detection.And to detect organic trace variation in the light-catalyzed reaction process, need to improve detection sensitivity by concentrating the thermal desorption technology.
(3) summary of the invention
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art part, a kind of new on-line automatic detection device be provided---light-catalyzed reaction-concentrated thermal desorption automatic sampling instrument.This device is combined as a whole reaction, sampling, sample concentration, desorb, sampling technique by automatic technology, can control reaction conditions automatically, as temperature of reaction, time, intensity of illumination; Automatically control sampling, sample injection time, sample size; Automatically control concentration time, desorption temperature, the desorption rate of sample; Can clean desorption apparatus automatically; Can with the chromatograph coupling, realize online reaction, online detection.
Concretely, light-catalyzed reaction of the present invention-concentrate the thermal desorption automatic sampling instrument to connect and compose jointly by photocatalytic reaction device, concentrated thermal desorption sampling device and control panel (Control Software is installed).Described photocatalytic reaction device is connected and composed jointly by light source, calandria A, thermopair A, photocatalytic coating, light-catalyzed reaction pipe, electromagnetic valve I, electromagnetic valve II, electromagnetic valve II I, electromagnetic valve I V, draft tube, carrier gas pipe A, blow-down pipe A and sample introduction pipe; Described concentrated thermal desorption sampling device is connected and composed jointly by thermal desorption cavity, calandria B, thermopair B, concentration tube, muff, solenoid valve V, solenoid valve VI, sample introduction needle, carrier gas pipe B and blow-down pipe B; Described control panel is electrically connected formation jointly by CPU microprocessor unit, driving circuit for electromagnetic valve, AC driving modules A～C, temperature signal A/D change-over circuit and RS232 serial communication circuit.Its mutual alignment and annexation are: light source is installed in light-catalyzed reaction inside pipe wall top in the photocatalytic reaction device, calandria A is installed in light-catalyzed reaction pipe outer wall, thermocouple A is installed in the light-catalyzed reaction pipe, draft tube, sample introduction pipe, carrier gas pipe A, blow-down pipe A are installed on the light-catalyzed reaction pipe, the solenoid valve I is installed on the draft tube, the solenoid valve II is installed on the carrier gas pipe A, the solenoid valve III is installed on the sample introduction pipe, the solenoid valve IV is installed on the blow-down pipe A, and photocatalytic coating is coated in light-catalyzed reaction pipe below inwall.Calandria B and thermopair B place in the thermal desorption cavity in the concentrated thermal desorption sampling device, concentration tube is installed in the thermal desorption cavity (putting into cavity by thermal desorption cavity upper aperture), the thermal desorption cavity is with muff outward, the thermal desorption cavity is circumscribed with carrier gas pipe B and blow-down pipe B, the solenoid valve V is installed on the blow-down pipe B, the solenoid valve VI is installed on the carrier gas pipe B, can select in the concentration tube to adorn adsorbents such as molecular sieve, acticarbon, silica gel, and in the thermal desorption cavity, directly be connected with the chromatographic injection port of external equipment by sample introduction needle.Photocatalytic reaction device is connected by the sample introduction pipe with concentrated thermal desorption sampling device, the input adapter of the output line of thermopair A and thermopair B and control panel A/D change-over circuit is electrically connected, the output interface of the incoming line of solenoid valve I～VI and control panel driving circuit for electromagnetic valve is electrically connected, the incoming line of light source, calandria A and calandria B is electrically connected with the output interface of control panel AC driving modules A, B and C respectively, and the RS232 serial communication circuit and the CPU microprocessor unit of control panel are electrically connected.
In foregoing invention, described CPU microprocessor unit is electrically connected jointly by CPU U1, capacitor C 1～C6, resistance R 1～R4 and crystal oscillator OSC1 and constitutes; Driving circuit for electromagnetic valve is electrically connected jointly by U4 Darlington driving array, hummer B1 and solenoid valve interface V1～V6 and constitutes; The AC driving module is electrically connected jointly and is constituted by K1, K2, three identical solid-state relays of K3 and J8～J10 interchange output driving interface; Temperature signal A/D change-over circuit is electrically connected jointly by U3A/D conversion chip, peripheral circuit C7～C14, resistance R 8 and crystal oscillator OSC2 and constitutes; The RS232 serial communication circuit is by the U5 level
Principle of work of the present invention is as follows: in the performance of research photocatalyst degraded organic volatile, the content that organism changes is micro-, absorption concentrates to organic volatile by selecting various solid adsorbent for use in the present invention, and the means of carrying out thermal desorption then improve detection sensitivity.Adopt collection, output, the reaction conditions of gas in the automated control technology control course of reaction simultaneously, make reaction, test integrated, realize online detection.
In the present invention, described photocatalytic reaction device directly is connected with concentrated thermal desorption sampling device, and by automatic control system, realizes reaction automatically, sampling automatically, concentrates automatically, desorb automatically, auto injection, cleans automatically.
In order to realize the present invention preferably, described muff adopts movable, can take away as required at any time, and temperature is reduced rapidly.
This light-catalyzed reaction-concentrate thermal desorption automatic sampling instrument can with gas chromatograph, gas-matter combined instrument or the gas chromatography-infrared spectrum combined instrument coupling of various models, make reaction, detection integrated, realize online detection.
The analysis field that the present invention is suitable for: environment monitoring, environmental assessment, catalysis material research, chemical industry and building materials field etc.
The present invention compared with prior art has the following advantages and effect:
(1) ability of measuring the catalysis material degradation of organic substances usually is to measure by gas chromatography, but since in this reaction organic concentration change very micro-, the trace that existing technology is difficult to detect in its course of reaction changes.The present invention adopts and concentrates the sensitivity that the thermal desorption technology has improved detection.
(2) reaction in the prior art, detection separate, and are difficult to realize online detection.Adopt automated control technology that photocatalytic reaction device and concentrated thermal desorption sampling device are combined, but realization response, detection robotization.The performance of the online detection catalysis material degradation of organic substances of energy is for the reaction of research photocatalysis to degrade organic matter provides a kind of strong means.
(3) in the design, the gas production of photocatalytic reaction device, supply gas, amount of reactant gases, reaction time be to control by computer software control electromagnetic valve I～V, the intensity of light source is by computer software control, temperature of reaction is to realize control automatically by computer software control calandria A, thermopair A, and entire reaction course can realize robotization.
(4) concentrate thermal desorption sampling device and adopt little stove formula structure, muff can be dismantled flexibly, can accelerate furnace temperature underspeeds, concentrate desorption temperature, the desorption time control able to programme of thermal desorption sampling device, be more suitable for the complex sample of desorb boiling range broad, and can in chromatograph, make the programmed temperature sampling device and use, can do cold focusing sample introduction, expand the functions of use of instrument.
(5) sample introduction needle directly is connected with the shortest path with the chromatograph injection port, reduces sample introduction space dead volume, makes sample that condensation, diffusion not take place.
(6) can carry out auto injection, and control the sample size of sample by the control sample injection time, both having solved gas sampler will be by changing the inconvenience that quantity tube changes sample size, solved the not enough shortcoming of syringe sampling accuracy again, more can guarantee sample when detecting stability and the reappearance of data.
(7) concentration tube can be equipped with the adsorbent of various performances as required, all can play best concentrated effect to different samples, and detection sensitivity is improved, and test specification is wider.
(8) photocatalytic reaction device and concentrated thermal desorption sampling device can clean automatically by software control solenoid valve VI, thereby reduce the sample cross pollution.
(4) description of drawings
Fig. 1 is the structured flowchart of light-catalyzed reaction-concentrated thermal desorption automatic sampling instrument.
Fig. 2 is the structural representation of photocatalytic reaction device.
Fig. 3 is the structural representation that concentrates thermal desorption sampling device.
Fig. 4 is the annexation synoptic diagram between circuit and the parts.
Fig. 5 is the circuit theory diagrams of control panel.
Fig. 6 is the FB(flow block) of Control Software.
(5) embodiment
Shown in Figure 1, light-catalyzed reaction of the present invention-concentrate the thermal desorption automatic sampling instrument to connect and compose jointly by photocatalytic reaction device, concentrated thermal desorption sampling device, control circuit (Control Software is installed).Photocatalytic reaction device is connected with concentrated thermal desorption sampling device, and control panel is connected with concentrated thermal desorption sampling device with photocatalytic reaction device, and by Control Software control photocatalytic reaction device and concentrated thermal desorption sampling device, thereby realize control automatically.
Shown in Figure 2, photocatalytic reaction device is connected and composed jointly by light source 1, calandria A2, electromagnetic valve I 3, electromagnetic valve II 4, electromagnetic valve II I5, electromagnetic valve I V6, light-catalyzed reaction pipe 7, photocatalytic coating 8, thermocouple A9, draft tube 10, sample introduction pipe 11, carrier gas pipe A12 and blow-down pipe A13.Described light source employing UV light source (10 ~ 40w), be mainly used in the light source that light-catalyzed reaction is provided; Described calandria A employing heater strip (50 ~ 200W), be mainly used in the temperature of regulating light-catalyzed reaction; Described solenoid valve flow is 20～200mL, flow rate of reactive gas when being used to control light-catalyzed reaction; Can adorn the film that scribbles photocatalyst (as photocatalyst of titanium dioxide of various variable concentrations etc.) in the described light-catalyzed reaction pipe, be used to study the ability of various photocatalyst for degrading organic volatiles.Photocatalytic reaction device is mainly used in realizes light catalase and mixed gas reaction.
Shown in Figure 3, concentrate thermal desorption sampling device and constitute by thermal desorption cavity 14, calandria B 15, thermopair B 16, muff 17, sample introduction needle 18, concentration tube 19, solenoid valve V 20, solenoid valve VI 21, carrier gas pipe B 22 and blow-down pipe B 23.Calandria B 15 and thermopair B 16 place in the thermal desorption cavity 14, are with muff 17 outside thermal desorption cavity 14.Thermal desorption cavity 14 outer carrier gas pipe B 22, solenoid valve V 21, blow-down pipe B 23 and the solenoid valve VI 20 of connecting, concentration tube 19 directly connects the chromatograph injection port by sample introduction needle 18 in thermal desorption cavity 14.Wherein: thermal desorption cavity 14 usefulness stainless steel materials are made, and are used to place calandria B 15, thermopair B 16, sample introduction needle 18 and concentration tube 19; Calandria B 15 selects 100～200W heating rod; Thermopair B 16 selects K type thermopair, is used to regulate the thermal desorption temperature; Muff 17 adopts dress heat-preservation cotton in the stainless steel casing, and is movable detachable, unloads the concentrated thermal desorption sampling device cooling rate of Shi Nengrang and accelerates; Sample introduction needle 18 can make the sample after the desorb directly enter chromatograph fast; Adsorbent (molecular sieve, acticarbon or silica gel etc.) is housed in the concentration tube 19; The flow range of solenoid valve V 20 is 5～50ml/min, is used to clean thermal desorption device, is realized by the computer settings scavenging period; The flow range of solenoid valve VI 21 is 5～50ml/min, is used to control sample size, realizes by the computer settings sample injection time.Concentrated thermal desorption sampling device mainly is to be used for the micro-organic component of concentration response gas, and it is determined that concentrated micro-organic component enters chromatograph by heating desorption.
Shown in Figure 4, control circuit on the control panel of the present invention is by CPU microprocessor unit, driving circuit for electromagnetic valve, AC driving modules A, AC driving module B, AC driving module C, and temperature signal A/D change-over circuit and RS232 serial communication circuit connect and compose jointly.Wherein the CPU microprocessor unit is by the temperature signal of A/D change-over circuit transition heat galvanic couple A 9 and thermopair B 15, and the data after will changing by the RS232 serial communication circuit are issued computing machine; Driving circuit for electromagnetic valve is used to drive solenoid valve I 3, solenoid valve II 4, solenoid valve III 5, solenoid valve IV 6 and solenoid valve V 20, solenoid valve VI 21; AC driving modules A, AC driving module B, AC driving module C are respectively applied for driving light source 1, calandria A 2 and calandria B 15.
Shown in Figure 5, the CPU microprocessor unit is electrically connected jointly by CPU U1, peripheral circuit C1～C6, resistance R 1～R4 and crystal oscillator OSC1 and constitutes; Driving circuit for electromagnetic valve is electrically connected jointly by Darlington driving array U4, hummer B1 and solenoid valve interface V1～V6 and constitutes; The AC driving module is electrically connected jointly and is constituted by K1, K2, three identical solid-state relays of K3 and J8～J10 interchange output driving interface; Temperature signal A/D change-over circuit is electrically connected jointly by A/D conversion chip U3, peripheral circuit C7～C14, resistance R 8 and crystal oscillator OSC2 and constitutes; The RS232 serial communication circuit is electrically connected jointly by level shifter interface chip U5 and peripheral circuit C15～C18 and constitutes.
Requiring of each parts is as follows: the optional PIC16C73 type of CPU microprocessor U1; Darlington drives the optional MC1413 type of array U4; Solid-state relay K1, K2, the optional GTJ3-2A type of K3; The optional AD7705 type of A/D conversion chip U3; The optional MAX232 type of RS232 serial port communication chip U5.
The major function of Control Software has:
(1) reaction time, light intensity, reaction unit temperature, the amount of reactant gases of control photocatalytic reaction device realize sampling, auto injection automatically.
(2) two kinds of type of heating of constant temperature, temperature programme of the concentrated thermal desorption sampling device of control, and sample injection time, scavenging period.
Figure 6 shows that Control Software controls the process flow diagram of photocatalytic reaction device automatically.
The process that adopts the present invention to detect automatically comprises the steps:
(1) at first this device is connected with chromatograph, opening device power supply and running gear Control Software are clicked " control automatically " pushbutton enable device and are entered automatic control state in the software control interface.
(2) in automatic control state, Control Software is opened electromagnetic valve I V and electromagnetic valve II automatically, logical nitrogen purge inside reactor, and this moment, electromagnetic valve II I and electromagnetic valve I were closed;
Close electromagnetic valve II after (3) 10 minutes, open electromagnetic valve I, charge into reacting gas 100ml, close electromagnetic valve I and electromagnetic valve I V then;
(4) electromagnetic valve II I is the switch that connects photocatalytic reaction device and concentrated thermal desorption sampling device gas circuit, open electromagnetic valve II, electromagnetic valve II I, open the solenoid valve V that concentrates on the thermal desorption sampling device simultaneously, quantitatively feed reacting gas to concentrating thermal desorption sampling device, feed the microcomponent in the concentration tube concentration response gas, close electromagnetic valve II, electromagnetic valve II I and solenoid valve V after 10 minutes;
(5) start heating function in the concentrated thermal desorption sampling device, open solenoid valve VI after the temperature balance, make the reacting gas that desorbs quantitatively feed gas chromatograph, concentrate thermal desorption sampling device prompting user this moment and start chromatograph analysis, this moment, measured value was the initial concentration of reaction gas before the light-catalyzed reaction; Open solenoid valve V set to be analyzed finishing such as analysis time by the user after, cleaned thermal desorption device automatically 10 minutes, close solenoid valve V and VI;
(6) repeating step (2) and (3);
(7) open reaction light source in the photocatalytic reaction device,, make the reaction of reacting gas and light catalase by computer software control intensity of illumination, temperature of reaction, reaction time;
(8) measure the concentration of light-catalyzed reaction afterreaction gas by above-mentioned steps (4) and (5),, can carry out the online detection that organic trace changes in the light-catalyzed reaction process so by the software control repetitive operation.
Apparatus of the present invention realize in the following way: earlier according to Fig. 2,3 processing equipment parts, press Fig. 5 processing circuit board, press Fig. 2,3,4 again and connect gas circuit and circuit part, and Control Software is installed.
Claims (4)
1. a light-catalyzed reaction-concentrate thermal desorption automatic sampling instrument, it is characterized in that: it is connected and composed jointly by photocatalytic reaction device, concentrated thermal desorption sampling device and control panel, and described photocatalytic reaction device is connected and composed jointly by light source (1), calandria A (2), thermopair A (9), photocatalytic coating (8), light-catalyzed reaction pipe (7), electromagnetic valve I (3), electromagnetic valve II (4), electromagnetic valve II I (5), electromagnetic valve I V (6), draft tube (10), carrier gas pipe A (12), blow-down pipe A (13) and sample introduction pipe (11); Described concentrated thermal desorption sampling device is connected and composed jointly by thermal desorption cavity (14), calandria B (15), thermopair B (16), concentration tube (19), muff (17), solenoid valve V (20), solenoid valve VI (21), sample introduction needle (18), carrier gas pipe B (22) and blow-down pipe B (23); Described control panel is electrically connected formation jointly by CPU microprocessor unit, driving circuit for electromagnetic valve, AC driving modules A～C, temperature signal A/D change-over circuit and RS232 serial communication circuit; Its mutual alignment and annexation are: light source in the photocatalytic reaction device (1) is installed in light-catalyzed reaction pipe (7) inwall top, calandria A (2) is installed in light-catalyzed reaction pipe (7) outer wall, thermocouple A (9) is installed in the light-catalyzed reaction pipe (7), draft tube (10), sample introduction pipe (11), carrier gas pipe A (12), blow-down pipe A (13) is installed on the light-catalyzed reaction pipe (7), electromagnetic valve I (3) is installed on the draft tube (10), electromagnetic valve II (4) is installed on the carrier gas pipe A (12), electromagnetic valve II I (5) is installed on the sample introduction pipe (11), electromagnetic valve I V (6) is installed on the blow-down pipe A (13), and photocatalytic coating (8) is coated in light-catalyzed reaction pipe (7) below inwall; Calandria B (15) and thermopair B (16) place in the thermal desorption cavity (14) in the concentrated thermal desorption sampling device, concentration tube (19) is installed in the thermal desorption cavity (14), the outer muff (17) that is with of thermal desorption cavity (14), thermal desorption cavity (14) is circumscribed with carrier gas pipe B (22) and blow-down pipe B (23), solenoid valve V (20) is installed on the blow-down pipe B (23), solenoid valve VI (21) is installed on the carrier gas pipe B (22), and concentration tube (19) directly is connected with the chromatographic injection port of external equipment by sample introduction needle (18) in thermal desorption cavity (14); Photocatalytic reaction device is connected by sample introduction pipe (11) with concentrated thermal desorption sampling device, the input interface of the output line of thermopair A (9) and thermopair B (16) and control panel A/D change-over circuit is electrically connected, the output interface of the incoming line of electromagnetic valve I～VI and control panel driving circuit for electromagnetic valve is electrically connected, the incoming line of light source (1), calandria A (2) and calandria B (15) is electrically connected with the output interface of control panel AC driving modules A, B and C respectively, and the RS232 serial communication circuit and the CPU microprocessor unit of control panel are electrically connected.
2. automatic sampling instrument as claimed in claim 1 is characterized in that: described CPU microprocessor unit is electrically connected jointly by CPU microprocessor U1, capacitor C 1～C6, resistance R 1～R4 and crystal oscillator OSC1 and constitutes; Driving circuit for electromagnetic valve is electrically connected jointly by Darlington driving array U4, hummer B1 and solenoid valve interface V1～V6 and constitutes; The AC driving module exchanges the output driving interface by three identical solid-state relays of K1, K2 and K3 and J8～J10 and is electrically connected jointly and constitutes; Temperature signal A/D change-over circuit is electrically connected jointly by A/D conversion chip U3, peripheral circuit C7～C14, resistance R 8 and crystal oscillator OSC2 and constitutes; The RS232 serial communication circuit is electrically connected jointly by level shifter interface chip U5 and capacitor C 15～C18 and constitutes.
3. automatic sampling instrument as claimed in claim 2 is characterized in that: described CPU microprocessor U1 adopts the PIC16C73 type; Darlington drives array U4 and adopts the MC1413 type; Solid-state relay K1, K2 and K3 adopt the GTJ3-2A type; A/D conversion chip U3 adopts the AD7705 type; Level shifter interface chip U5 adopts the MAX232 type.
4. as claim 1 or 2 or 3 described automatic sampling instruments, it is characterized in that: described light source adopts 10～40W UV light source; Described calandria A adopts the heater strip of 50～200W, and calandria B adopts the heating rod of 100～200W; The flow range of described solenoid valve I～IV is 20～200mL, and the flow range of solenoid valve V～VI is 5～50ml/min; Described photocatalytic coating is the film that scribbles the variable concentrations photocatalyst of titanium dioxide; Thermopair B is a K type thermopair; Muff adopts dress heat-preservation cotton in the stainless steel casing, and is movable detachable; Sorbent molecule sieve, acticarbon or silica gel are housed in the described concentration tube.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2007100290593A CN101082611B (en) | 2007-07-06 | 2007-07-06 | light-catalyzed reaction concentrating thermal decomposition suction automatic sampling instrument |
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| CN2007100290593A CN101082611B (en) | 2007-07-06 | 2007-07-06 | light-catalyzed reaction concentrating thermal decomposition suction automatic sampling instrument |
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| CN101082611B true CN101082611B (en) | 2011-02-23 |
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| CN106383165A (en) * | 2016-12-07 | 2017-02-08 | 邯郸学院 | Method for continuously measuring reaction speed of carbon-containing solid substances such as coal |
| CN108760958A (en) * | 2018-07-02 | 2018-11-06 | 东华理工大学 | The light-catalyzed reaction on-line detecting system of self-priming automatic sampling |
| CN111905672B (en) * | 2020-06-22 | 2021-10-08 | 西安交通大学 | Multichannel continuous online detection photocatalysis reaction device |
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